利用高效液相色谱-质谱法同时测定药物饲料中的磺胺类药物、三甲氧苄啶、阿莫西林和泰乐菌素。

IF 1.3 3区 农林科学 Q2 VETERINARY SCIENCES Journal of Veterinary Research Pub Date : 2024-03-23 eCollection Date: 2024-03-01 DOI:10.2478/jvetres-2024-0011
Ewelina Patyra, Krzysztof Kwiatek
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引用次数: 0

摘要

简介文章介绍了测定动物药用饲料中四种磺胺类药物(磺胺嘧啶、磺胺二甲嘧啶、磺胺甲噁唑和磺胺甲噁唑)、三甲氧苄啶、泰乐菌素和阿莫西林的快速而简单的分析程序:对 18 份药物饲料样本进行了活性物质分析。分析方案使用乙腈和 0.05 M 磷酸缓冲液(pH 值为 4.5)的混合物提取七种抗菌物质。萃取后的样品用 Milli-Q 水稀释,然后用液相色谱-质谱法进行分析。从线性、选择性、定量限和测定限、重复性、再现性和不确定性等方面对所开发的程序进行了验证:根据欧盟委员会实施条例(EU)2021/808 和 ICH 指南中规定的标准对该方法进行了验证。该方法的平均回收率为 90.8%-104.5%,所有分析抗菌物质的重复性和再现性变异系数分别为 3.2%-6.9%和 5.2%-8.3%。所有七种分析物的检出限和定量限分别为 5.4 mg/kg 至 48.3 mg/kg 和 10.4 mg/kg 至 119.3 mg/kg。根据化合物的不同,方法的不确定度从14.0%到24.0%不等。该方法成功地应用于 18 种药物饲料:结论:所开发的方法可成功用于常规控制药物饲料中七种抗菌物质的含量和均一性。
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Simultaneous determination of sulfonamides, trimethoprim, amoxicillin and tylosin in medicated feed by high performance liquid chromatography with mass spectrometry.

Introduction: The article presents a rapid and simple analytical procedure for determination of four sulfonamides (sulfadiazine, sulfamerazine, sulfamethazine and sulfamethoxazole), trimethoprim, tylosin and amoxicillin in animal medicated feed.

Material and methods: Eighteen medicated feed samples were analysed for active substances. The analytical protocol used a mixture of acetonitrile and 0.05 M phosphoric buffer, pH 4.5 for the extraction of seven antibacterial substances. After extraction, the samples were diluted in Milli-Q water and analysed by liquid chromatography with mass spectrometry. The developed procedure was subjected to validation in terms of linearity, selectivity, limits of quantification and determination, repeatability, reproducibility and uncertainty.

Results: The validation of the method was carried out in accordance with the criteria set out in Commission Implementing Regulation (EU) 2021/808 and ICH guidelines. This method provided average recoveries of 90.8 to 104.5% with coefficients of variation for repeatability and reproducibility in the ranges of 3.2-6.9% and 5.2-8.3%, respectively for all analysed antibacterial substances. The limit of detection and limit of quantification for all seven analytes ranged from 5.4 mg/kg to 48.3 mg/kg and from 10.4 mg/kg to 119.3 mg/kg, respectively. The uncertainty of the method depending on the compound varied from 14.0% to 24.0%. The validated method was successfully applied to the 18 medicated feeds.

Conclusion: The developed method can be successfully used to routinely control the content and homogeneity of seven antibacterial substances in medicated feed.

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来源期刊
Journal of Veterinary Research
Journal of Veterinary Research Veterinary-General Veterinary
CiteScore
0.90
自引率
5.60%
发文量
58
审稿时长
18 weeks
期刊介绍: Journal of Veterinary Research (formerly Bulletin of the Veterinary Institute in Pulawy) is a quarterly that publishes original papers, review articles and short communications on bacteriology, virology, parasitology, immunology, molecular biology, pathology, toxicology, pharmacology, and biochemistry. The main emphasis is, however, on infectious diseases of animals, food safety and public health, and clinical sciences.
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